Novel crystal form cetilistat and preparation method thereof

A technology of celistat and its crystal form, which is applied in the field of crystallization of pharmaceutical compounds, can solve the problems of unsuitability for large-scale industrial production, cumbersome operation steps, and long preparation time, and achieve excellent stability, simple process, and good reproducibility Effect

Inactive Publication Date: 2015-12-02
JINAN KANGHE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The present invention is a new crystal of selista proposed for the problems of cumbersome operation steps in the preparation process of the above two crystal forms A and B, long preparation time, high toxicity of solvents used and unsuitability for large-scale industrial production. type and its preparation method

Method used

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  • Novel crystal form cetilistat and preparation method thereof
  • Novel crystal form cetilistat and preparation method thereof
  • Novel crystal form cetilistat and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Preparation of new crystal form of Selista

[0038] The crude product of Selistat was prepared according to the route described in the patent US2003027821A.

[0039] 1) The preparation method of the new crystal form of Selista is as follows:

[0040] (1) Add 10 g of the crude selestat obtained by the above method into absolute ethanol, wherein the mass ratio of the crude selestat to absolute ethanol is 1:6, heat up to 45° C. and stir to dissolve;

[0041] (2) After dissolving, cool down to 10°C for crystallization at a cooling rate of 10°C / h, and stir at this temperature for 0.5 hours to obtain crystallization;

[0042] (3) Filtration, washing with absolute ethanol, and air-drying at 30° C. for 4 hours to obtain 8.8 g of the new crystal form of selista, with a yield of 88.0%.

[0043] After testing, the melting point of the new crystal form of Selista is 73.5-74.8°C.

[0044] 2) Detection conditions and results

[0045] (1) The X-ray powder diffraction te...

Embodiment 2

[0060] Embodiment 2: Preparation of new crystal form of Selista

[0061] The crude product of Selistat was prepared according to the route described in the patent US2003027821A.

[0062] 1) The preparation method of the new crystal form of Selista is as follows:

[0063] (1) Add 10 g of the crude selestat obtained by the above method into methanol, wherein the mass ratio of the crude selestat to methanol is 1:5, heat up to 50° C. and stir to dissolve;

[0064] (2) After dissolving, cool down to 15°C at a cooling rate of 10°C / h to crystallize, and stir at this temperature for 0.5 hours to obtain crystallization;

[0065] (3) Filtration, washing with methanol, and air-drying at 30° C. for 4 hours to obtain 8.5 g of the new crystal form of selistastat with a yield of 85.0%.

[0066] After testing, the melting point of the new crystal form of Selista is 73.6-74.7°C.

[0067] 2) Detection conditions and results

[0068] The instrument used in this embodiment is the same as embo...

Embodiment 3

[0074] Example 3: Preparation of new crystal form of Selista

[0075] The crude product of Selistat was prepared according to the route described in the patent US2003027821A.

[0076] The preparation method of the new crystal form of Selista is as follows:

[0077] (1) Add 10 g of the crude selestat obtained by the above method into ethyl acetate, wherein the mass ratio of the crude selestat to ethyl acetate is 1:3, heat up to 55° C. and stir to dissolve;

[0078] (2) After dissolving, cool down to 12°C to crystallize at a cooling rate of 20°C / h, and stir at this temperature for 0.5 hours to obtain crystallization;

[0079] (3) Filtration, washing with ethyl acetate, and air-drying at 30°C for 4 hours to obtain 8.6 g of the new crystalline form of selestat, with a yield of 86.0%.

[0080] After testing, the melting point of the new crystal form of Selista is 73.5-74.9°C.

[0081] The instrument used in this embodiment is the same as that in Example 1.

[0082] As detected ...

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Abstract

The invention relate to a crystal form of cetilistat, in particular to novel crystal form cetilistat and a preparation method thereof. The novel crystal form cetilistat is characterized in that X-ray powder diffraction expressed via Cu-Ka radiation at an angle 2Theta has characteristic peaks at 3.77+ / -0.2, 4.25+ / -0.2, 7.71+ / -0.2, 8.67+ / -0.2, 10.59+ / -0.2 and 23.7.71+ / -0.2. The invention further provides a preparation method of the novel crystal form cetilistat; the preparation method is simple, is easy to operate, good in reproducibility and high in purity, takes short time and consumes lower energy under dryness condition, and a solvent for use is low in toxicity. The novel crystal form cetilistat has better stability and is more suitable for uses in the predation of compositions used for treating obesity.

Description

technical field [0001] The invention relates to the field of pharmaceutical compound crystallization, in particular to a new crystal form of Selistat and a preparation method thereof. Background technique [0002] Cetilistat (cetilistat), also known as new lixistat, cetilistat, chemical name: 2-hexadecyloxy-6-methyl-4 hydrogen-3,1-benzoxazine- 4-keto, a new gastrointestinal lipase inhibitor for the treatment of obesity and type II diabetes. It was first developed by the British company Alizyme, and later jointly developed by the Dutch Norgine company and the Japanese Takeda company, and was approved to be listed in Japan. The compound has the following structural formula: [0003] [0004] At present, the method for preparing Selistat mainly contains the following two routes: [0005] Route 1 refers to the patent US2003027821A, using cetyl alcohol as the starting material, preparing hexadecyl chloroformate through phosgene, and then reacting with 2-amino-5-methylbenzoi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/26A61P3/04
CPCC07D265/26C07B2200/13
Inventor 张颖高国锐徐英军孙丽梦
Owner JINAN KANGHE MEDICAL TECH
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